RU2227170C1 - Method of extraction of rhenium - Google Patents

Abstract

FIELD: hydrometallurgy. SUBSTANCE: proposed method includes sorption of rhenium by granulated polymer, de-sorption of rhenium ammonium solvent for obtaining rhenium-concentrated solutions. Used as sorbent is extracting polymer containing super-cross-linked polystyrene and extracting agent. Used as extracting agent is trialkylamine of the following formula: R₃N, where R are alkyl radicals (C₈-C₁₀). Granules of super-cross-linked polystyrene are impregnated by use of 0.1=40-% solution of trialkylamine of formula R₃N, where R is alky radicals (C₈-C₁₀) in organic diluent. EFFECT: high degree of extraction of rhenium from weak solutions; reduction of time required for process; low cost. 4 tbl, 2 ex 5

Description

The invention relates to hydrometallurgy and can be used to extract rhenium from solutions.

Known methods for the extraction of rhenium by sorption using strongly [1] and weakly basic [2] ion exchange resins.

The disadvantage of these extraction methods is the low selectivity in the extraction of rhenium from industrial solutions containing, in addition to rhenium (from 0.05 to 0.2 g / l) to 25 g / l of molybdenum and other impurities. In order to effectively separate Re and Mo, it is necessary to strictly control the pH of the processed solutions and use concentrated acids in the technology, as well as the slow kinetics of mass transfer of ReO ions $\genfrac{}{}{0ex}{}{\text{-}}{\text{4}}$ in sorbents, reaching several hours. The industrial use of the above ion-exchange resins is constrained by the high cost and large volumes of purchases of ion-exchange resins needed to create industrial plants for the extraction of rhenium from solutions with a content of Re <10 mg / L.

Closest to the proposed technical essence is a method for extracting rhenium on a granular polymer [3], in which anion exchange resin AN-21 of a porous modification containing 16% divinibenzene as a crosslinking agent and 0.8-1.0 wt.h. . isooctanol as a blowing agent. In this method of rhenium extraction, a soda desorbate of the following composition: 435-760 Re; 110-140 SO $\genfrac{}{}{0ex}{}{\text{2-}}{\text{4}}$ ; 700-800 Cl ^- , acidified to pH 4 with hydrochloric acid, was sent to ion-exchange columns. Sorption was carried out until the rhenium passed through in the filtrate, 230-250 mg / L; rhenium was eluted from the saturated resin with a heated ammonia solution of 2.6-2.7 N at a temperature of 40 ° С.

The disadvantages of this method of rhenium extraction can be attributed to the mandatory acidification of solutions with hydrochloric acid before sorption, which dramatically increases production costs with large volumes of processed solutions. The minimum elution time is 5-6 hours, and the entire technological cycle of the rhenium extraction technology on the AN-21 ion-exchange resin is 25-30 hours, which greatly complicates the entire technological process for producing rhenium-containing salts. Moreover, for the complete elution of rhenium from the resin, 10 specific volumes of the eluate are required.

The technical result of the invention is that the sorption and desorption time compared with the same indicators of the known rhenium sorbents ASBR-1, AN-21 (p), VP-14KR is significantly reduced, which dramatically reduces and reduces the cost of the hardware circuit and technology in the processing of poor rhenium-containing solutions (with a concentration of ≤ 10 mg / l rhenium).

The technical result is achieved by the fact that in the method for extracting rhenium from solutions, including sorption of rhenium by a granular polymer, desorption of rhenium with an ammonia solution to obtain rhenium concentrated solutions, granules of hypercrosslinked polystyrene impregnated in a 0.1-40% solution of trialkylamine of the general formula are used as a sorbent R ₃ N, where R is C ₈ -C ₁₀ alkyl radicals in an organic solvent.

The minimum and maximum amount of extractant (from 0.1 to 40%) is selected on the basis that less than 0.1% the extraction ability of a multicomponent polymer is sharply reduced. At extractant concentrations above 40%, the loss of extractant from the polymer matrix sharply increases during rhenium extraction.

The extracting polymer (EP), proposed for rhenium extraction, has an increased resistance to abrasion (it exceeds the strength of the currently used ion-exchange resins made on the basis of DVB divinylbenzene and vinylpyridine (Table 2)). The entrainment of extractant from EP granules over 10 cycles was not observed. The capacity for rhenium in the proposed sorbent did not change (table 1).

The invention was carried out as follows.

Example. Rhenium was extracted from solutions containing 10.23 mg / dm ^{3 of} rhenium and 110 g / dm ^{3 of} sulfuric acid under static conditions. In a beaker with a mixer was placed 1 g of granular extracting polymer (EP) with a diameter of granules of 0.4 mm, with different concentrations of TAA (see table) and 0.5 dm ^{3 of} rhenium-containing solution. The mass transfer rate during the extraction of rhenium from sulfuric acid solutions significantly exceeds the currently used sorbents AMP, AN-21 (p), VP-14KR and does not exceed 120 minutes (Table 3). Analyzes for the content of rhenium was carried out according to the standard method colorimetric method.

Rhenium was regenerated from saturated EP, AMP, VP-14KR by a solution containing 10% ammonia, and was carried out in one stage. The rhenium-saturated polymer was mixed with 20 ml of a regenerating solution in a beaker with a mechanical stirrer for 15, 30, 70, and 90 minutes (Table 4). Part of the solution was selected for analysis. The extracting polymer was filtered off, washed with distilled water at a ratio of T: L = 1: 10, and regenerated with 10% ammonia at a ratio of T: L = 1: 20.

From the results given in table 4, it follows that the application of the claimed method of extracting rhenium from solutions will allow:

- provide a high degree of extraction of rhenium from poor solutions;

- reduce the time of the entire technological cycle sorption - regeneration of rhenium up to 2 hours;

- due to the low losses of EP in cycles, reduce the cost of the technology for extracting rhenium from solutions by several times by reducing the amount of EP used in the sorbent necessary for the entire technological cycle;

- it is economically viable to extract rhenium from solutions of underground leaching (PV), heap leaching (KB), volcanic origin, etc. with rhenium content <1 mg / dm ³ .

SOURCES OF INFORMATION

1. V.I. Bibikova, A.V. Peredereev et al. Kinetics of the ion exchange of rhenium and molybdenum on resin AM./ In Sat. "Rhenium. Chemistry, technology, analysis. ” - M .: Nauka, 1976, p. 54-60.

2. A.G. Kholmogorov et al. Extraction of rhenium from sulfuric acid solutions and its separation from molybdenum on various types of anion exchangers - Ibid., Pp. 63-66.

3.K.B. Lebedev et al. Industrial testing and introduction of anion-21 AN-21 porous modification for rhenium extraction. // Non-ferrous metals, No. 2, 1976, p. 79-83.

Claims (1)

A method for extracting rhenium from solutions, including sorption of rhenium by a granular polymer, desorption of rhenium with an ammonia solution to obtain rhenium concentrated solutions, characterized in that granules of hypercrosslinked polystyrene impregnated in a 0.1-40% solution of trialkylamine of the general formula R ₃ N are used as sorbent where R-alkyl radicals of C ₈ -C ₁₀ in an organic solvent.